CN101570462B - Fischer-Tropsch synthesis method - Google Patents
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- CN101570462B CN101570462B CN 200810105614 CN200810105614A CN101570462B CN 101570462 B CN101570462 B CN 101570462B CN 200810105614 CN200810105614 CN 200810105614 CN 200810105614 A CN200810105614 A CN 200810105614A CN 101570462 B CN101570462 B CN 101570462B
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Abstract
The invention relates to a Fischer-Tropsch synthesis method, which comprises that: hydrogen and carbon monoxide contact with each other under the condition of Fischer-Tropsch synthesis and in the presence of a Fischer-Tropsch synthesis catalyst, wherein the Fischer-Tropsch synthesis catalyst comprises a first Fischer-Tropsch synthesis catalyst and a second Fischer-Tropsch synthesis catalyst; the pore volume of the first Fischer-Tropsch synthesis catalyst is less than that of the second Fischer-Tropsch synthesis catalyst; and the hydrogen and the carbon monoxide contact with the first Fischer-Tropsch synthesis catalyst first and then contact with the second Fischer-Tropsch synthesis catalyst. By making the hydrogen and the carbon monoxide contact with the first Fischer-Tropsch synthesis catalyst with small pore volume first and then contact with the second Fischer-Tropsch synthesis catalyst with large pore volume, the method can give full play to the catalysis of the catalyst, reduce the selectivity of CH4 products, improve the selectivity of a Fischer-Tropsch synthesis liquid C5+ hydrocarbon, and simultaneously improve the conversion rate of raw materials CO.
Description
Technical field
The present invention relates to a kind of Fischer-Tropsch synthesis method.
Background technology
Contain hydrocarbon resource and go out synthetic gas as raw material production so that Sweet natural gas, pitch, coal, biomass etc. are various, again take synthetic gas as raw material by the synthetic liquefied hydrocarbon of producing of Fischer-Tropsch, be a good oil replacement technology.Fischer-Tropsch synthetic (Fischer-Tropsch synthesis) is synthetic take the technological process of paraffinic hydrocarbon as main liquid fuel under catalyzer (mainly being iron system) and appropriate reaction condition take synthetic gas as raw material.Nineteen twenty-three is executed exploitation by Germanization scholar F. Fischer and H. Toro are general, the during World War II scale production that has high input.Its reaction process can represent with following formula:
nCO+2nH
2→[CH
2]
n+nH
2O
But traditional Fischer-Tropsch synthesis method is take cobalt as catalyzer, and products obtained therefrom forms complicated, poor selectivity, and light liquid hydrocarbons is few, and the heavy paraffinic hydrocarbon is more.Its main component is straight-chain paraffin, alkene, a small amount of aromatic hydrocarbons and by-product water and carbonic acid gas.In decades, the synthetic study hotspot of Fischer-Tropsch is to strengthen synthetic selectivity, improves to contain the productive rate that carbon number is the hydro carbons of required numerical range.Generally speaking, C
5+ liquefied hydrocarbon is needed product.
US 6765026B2 provides a kind of Fischer-Tropsch synthesis method that special catalyst carries out catalysis of using.The presoma of the method catalyst system therefor is the soluble compounds of a kind of iron group (especially cobalt) metal or soluble compounds or the salt of salt and a kind of VIII family's metal (especially platinum).The solution of presoma with hydroxyhy-drocarbyl amines or ammonium hydroxide is contacted, obtain a kind of special catalyzer.Utilize this catalyzer can obtain beyond thought highly selective catalytic effect, make C
5The selectivity of+hydro carbons reaches the 58-80 % by weight.But, use the method gaseous product CH
4Selectivity to be about the transformation efficiency of 10%, CO still not high.Thereby, need to propose new Fischer-Tropsch synthesis method with further raising C
5The selectivity of+hydro carbons and reduction CH
4Selectivity, improve the transformation efficiency of raw material CO.
Summary of the invention
The object of the invention is to overcome Fischer-Tropsch synthesis C in the prior art
5+ hydrocarbon selective deficiency and CH
4Selectivity high, the shortcoming of CO low conversion rate provides a kind of C
5High and the CH of+hydrocarbon selective
4The Fischer-Tropsch synthesis method that selectivity is low and the CO transformation efficiency is high.
The invention provides a kind of Fischer-Tropsch synthesis method, the method is included in fischer-tropsch synthetic catalyst and exists lower, hydrogen is contacted with CO (carbon monoxide converter) gas, wherein, described fischer-tropsch synthetic catalyst comprises the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst, the pore volume of the first fischer-tropsch synthetic catalyst is less than the pore volume of the second fischer-tropsch synthetic catalyst, and hydrogen contacts with the first fischer-tropsch synthetic catalyst first with CO (carbon monoxide converter) gas, contacts with the second fischer-tropsch synthetic catalyst again.
Method of the present invention contacts hydrogen and CO (carbon monoxide converter) gas first with less the first fischer-tropsch synthetic catalyst of pore volume, contact with larger the second fischer-tropsch synthetic catalyst of pore volume again, can give full play to the katalysis of catalyzer, reduction product C H
4Selectivity, improve Fischer-Tropsch synthetic fluid C
5The selectivity of+hydro carbons improves the transformation efficiency of raw material CO simultaneously.
Description of drawings
Fig. 1 is Fischer-Tropsch synthesis method schematic diagram provided by the invention.
Embodiment
Fischer-Tropsch synthesis method provided by the invention is included in fischer-tropsch synthetic catalyst and exists lower, hydrogen is contacted with CO (carbon monoxide converter) gas, wherein, described fischer-tropsch synthetic catalyst comprises the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst, the pore volume of the first fischer-tropsch synthetic catalyst is less than the pore volume of the second fischer-tropsch synthetic catalyst, hydrogen contacts with the first fischer-tropsch synthetic catalyst first with CO (carbon monoxide converter) gas, contacts with the second fischer-tropsch synthetic catalyst again.
The pore volume of described the first fischer-tropsch synthetic catalyst can be 0.1-1 ml/g, is preferably 0.2-0.5 ml/g, and the pore volume of the second fischer-tropsch synthetic catalyst can be 0.1-1 ml/g, is preferably 0.5-1 ml/g.And the difference of the pore volume of the pore volume of the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst is 0.1-0.7 ml/g.
Take the cumulative volume of the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst as benchmark, the loadings of described the first fischer-tropsch synthetic catalyst can be 10-90 volume %, be preferably 30-70 volume %, the loadings of the second fischer-tropsch synthetic catalyst can be 10-90 volume %, is preferably 30-70 volume %.
The present invention is not particularly limited composition and the kind of the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst.The catalyzer that any routine is used for the catalysis Fischer-Tropsch synthesis all can be used as the first fischer-tropsch catalysts and/or the second fischer-tropsch catalysts, as long as the pore volume that makes the first fischer-tropsch synthetic catalyst is than the little 0.1-0.7 of pore volume ml/g of the second fischer-tropsch synthetic catalyst.Under the preferable case, the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst are respectively and contain heat-resisting inorganic materials carrier and the cobalt and/or the cobalt compound that load on this carrier.
In described the first fischer-tropsch synthetic catalyst, take the gross weight of the first fischer-tropsch synthetic catalyst as benchmark, in oxide compound, the content of cobalt is the 5-20 % by weight; In described the second fischer-tropsch synthetic catalyst, take the gross weight of the second fischer-tropsch synthetic catalyst as benchmark, in oxide compound, the content of cobalt is the 1-20 % by weight.Wherein, the compound of described cobalt is cobalt oxide and/or solubility cobalt salt, and described heat-resisting inorganic materials is selected from one or more in aluminum oxide, pure aluminium silicate, silicon oxide, titanium oxide, zirconium white, the gac.
The specific surface area of the carrier of described the first fischer-tropsch synthetic catalyst can be the 50-400 meters squared per gram, be preferably the 100-300 meters squared per gram, the specific surface area of the carrier of the second fischer-tropsch synthetic catalyst can be the 100-400 meters squared per gram, is preferably the 100-300 meters squared per gram.
Described Fischer-Tropsch synthesis condition comprises that the pressure that hydrogen contacts with CO (carbon monoxide converter) gas can be the 0.5-6 MPa, is preferably the 2-4 MPa; The temperature of contact can be 150-350 ℃, is preferably 180-220 ℃; Gas hourly space velocity can be 200-3000 hour
-1, be preferably 400-1000 hour
-1, the raw materials components mole ratio of hydrogen and CO (carbon monoxide converter) gas can be 1-3: 1, be preferably 1.8-2.2: 1.
Fischer-tropsch synthetic catalyst of the present invention can be divided into several according to the pore volume size, as long as its kind number is not less than 2, that is: except described the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst, the fischer-tropsch synthetic catalyst that can also comprise other kind, as long as the 30 volume % or the above and hydrogen that make the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst account for respectively the catalyzer cumulative volume contact with the second fischer-tropsch synthetic catalyst with the first fischer-tropsch synthetic catalyst successively with CO (carbon monoxide converter) gas, the putting in order of catalyzer of other pore volume that selectivity is contained is not particularly limited.
Described catalyzer carry out Fischer-Tropsch synthetic before, at first in hydrogen atmosphere, carry out reduction activation.Reduction activation was carried out under 200-900 ℃ temperature 0.5-96 hour, was preferably 2-30 hour.The mixture that adopts hydrogen and nitrogen or rare gas element in this reduction activation process is as medium, and wherein density of hydrogen is 1-100 volume %.The pressure of reducing atmosphere is the 0.01-4.0 MPa, preferred 0.01-1.0 MPa; Gas hourly space velocity is 100-2000 hour during reduction
-1, preferred 300-1000 hour
-1
Fig. 1 is Fischer-Tropsch synthesis method schematic diagram provided by the invention.Below in conjunction with accompanying drawing method provided by the present invention is further described, has omitted among the figure and well known to a person skilled in the art such as equipment such as pump, interchanger, compressors.
Fischer-Tropsch synthesis method technical process provided by the invention is described below:
H
2Enter Fischer-Tropsch synthesis device 3 so that the certain proportion mixing is rear by feeding line 1 with CO, at first enter the first reaction zone A and contact with the first fischer-tropsch synthetic catalyst, under the effect of the first catalyzer, carry out Fischer-Tropsch synthesis; Resultant of reaction enters second reaction zone B with unreacted unstripped gas and contacts with the second fischer-tropsch synthetic catalyst, proceeds Fischer-Tropsch synthesis under the effect of the second catalyzer.Resultant of reaction and unreacted unstripped gas flow out from reactor bottom, enter high pressure hot separator 5 through transfer line 4.In high pressure hot separator 5, carry out feed separation, high boiling liquid hydro carbons and part water enter thermal low-pressure separators 7 through liquid product pipeline 6, hydro carbons further separates with water in thermal low-pressure separators 7, hydro carbons is flowed out as output of products by gaseous product outlet 8, and water is through water discharge line 9 discharge systems.In high pressure hot separator 5, the low boiling point hydrocarbon of unreacted unstripped gas, generation and part water enter cold high pressure separator 11 through gas transmission line 10 and carry out gas-liquid separation, the gas part enters reactor through feed back pipeline 13 and further participates in Fischer-Tropsch synthesis, rest part is through venting port 12 discharge systems, liquid portion enters cold low separator 15 through tapping line 14 and isolates low-boiling point liquid hydro carbons and water, wherein as output of products, water is through water outlet 17 discharge systems by hydrocarbon stream outlet 16 for the low-boiling point liquid hydro carbons.
The present invention will be described in more detail below in conjunction with embodiment.
Prepare the aqueous solution that contains Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 65 gram in per hundred ml solns, adopt the saturated pickling process in hole, use this solution impregnation of alumina carrier, 600 ℃-1050 ℃ of the maturing temperatures of alumina supporter wherein are afterwards in 120 ℃ of dryings 3 hours.Roasting is 3 hours under 350 ℃ of-450 ℃ of differing tempss, and temperature rise rate is 3 ℃/minute, obtains the catalyzer of different pore volumes.The catalyst activity evaluation is carried out in fixed-bed reactor.
Measure the pore volume of catalyzer with the BET method.
Embodiment 1
The present embodiment is used for illustrating Fischer-Tropsch synthesis method provided by the invention.
Device as shown in Figure 1, the first reaction zone A loads the first fischer-tropsch synthetic catalyst at reactor, loads the second fischer-tropsch synthetic catalyst at second reaction zone B.Wherein, the pore volume of the first fischer-tropsch synthetic catalyst is 0.4 ml/g (950 ℃ of carrier maturing temperatures, 400 ℃ of catalyzer maturing temperatures), take the gross weight of the first catalyzer as benchmark, the content of cobalt oxide is 14 % by weight, and carrier is aluminum oxide, and specific surface area is 200 meters squared per gram.The pore volume of the second fischer-tropsch synthetic catalyst is 0.6 ml/g of (900 ℃ of carrier maturing temperature, 400 ℃ of catalyzer maturing temperatures), take the gross weight of the second catalyzer as benchmark, the content of cobalt oxide is 14 % by weight, carrier is aluminum oxide, and specific surface area is 180 meters squared per gram.The volume of the first catalyzer and the second catalyzer equates.Catalyzer at first passes into pure hydrogen reductase 12 4 hours under 400 ℃, then pass into synthetic gas and carry out Fischer-Tropsch synthesis.Synthetic reaction condition is: 208 ℃ of temperature, pressure 2.5 MPas, gas hourly space velocity 500 hours
-1, H
2With the raw materials components mole ratio of CO be 2: 1.
Embodiment 2
The present embodiment is used for illustrating Fischer-Tropsch synthesis method provided by the invention.
According to method similarly to Example 1, different is, the pore volume of the first fischer-tropsch synthetic catalyst is 0.2 ml/g of (1050 ℃ of carrier maturing temperature, 400 ℃ of catalyzer maturing temperatures), the pore volume of the second fischer-tropsch synthetic catalyst is 0.9 ml/g of (700 ℃ of carrier maturing temperature, 400 ℃ of catalyzer maturing temperatures), and the volume ratio of the first catalyzer and the second catalyzer be 7: 3.
Embodiment 3
The present embodiment is used for illustrating Fischer-Tropsch synthesis method provided by the invention.
According to method similarly to Example 1, different is, the pore volume of the first fischer-tropsch synthetic catalyst is 0.3 ml/g of (980 ℃ of carrier maturing temperature, 400 ℃ of catalyzer maturing temperatures), the pore volume of the second fischer-tropsch synthetic catalyst is 0.7 ml/g of (800 ℃ of carrier maturing temperature, 400 ℃ of catalyzer maturing temperatures), and the volume ratio of the first catalyzer and the second catalyzer be 3: 7.
Comparative Examples 1
This Comparative Examples is used for explanation prior art Fischer-Tropsch synthesis method.
According to the method identical with embodiment 1, different is only to load a kind of catalyzer in the Fischer-Tropsch synthesis device 3.The pore volume of this catalyzer is 0.4 ml/g, and take the gross weight of catalyzer as benchmark, the content of cobalt oxide is 14 % by weight, and carrier is aluminum oxide, and specific surface area is 190 meters squared per gram.
Comparative Examples 2
This Comparative Examples is used for explanation prior art Fischer-Tropsch synthesis method.
According to the method identical with embodiment 1, different is only to load a kind of catalyzer in the Fischer-Tropsch synthesis device 3.The pore volume of this catalyzer is 0.6 ml/g, and take the gross weight of catalyzer as benchmark, the content of cobalt oxide is 14 % by weight, and carrier is aluminum oxide, and specific surface area is 190 meters squared per gram.
Result's test
Measure respectively CO in the gaseous product, CH with vapor-phase chromatography
4And C
2-C
4The amount of product, and calculate its mole number.To deduct as the amount of the CO of raw material the amount that transforms the CO that falls that measures of remaining CO.The mole number that transforms the CO that falls deducts CH in the gaseous product
4And C
2-C
4The mole number of middle C can obtain C
5The mole number of the C of+product.
The CO transformation efficiency refers to react the ratio that the CO quantity of falling accounts for the CO total feed that transforms.CH
4Selectivity refers to generate CH
4Required C mole number accounts for the mole number of the CO that reacts away.C
5+ selectivity refers to generate C
5The C mole number of+product accounts for the mole number of the CO that reacts away.Test result is listed in table 1.
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| The CO transformation efficiency | 91.95 | 91.68 | 92.07 | 91.52 | 90.65 |
| CH 4Selectivity/% | 8.36 | 8.79 | 8.52 | 9.35 | 10.03 |
| C 5 +Selectivity/% | 82.85 | 82.51 | 82.63 | 81.16 | 80.25 |
Contrast table 1 listed test result can be found out, adopts method provided by the invention to carry out the Fischer-Tropsch synthesis product C
5+ liquid hydrocarbon selectivity is high, CH
4Selectivity is low and the CO transformation efficiency is high.
Claims (7)
1. Fischer-Tropsch synthesis method, the method is included under the Fischer-Tropsch synthesis condition and fischer-tropsch synthetic catalyst exists lower, hydrogen is contacted with CO (carbon monoxide converter) gas, it is characterized in that, described fischer-tropsch synthetic catalyst comprises the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst, the pore volume of the first fischer-tropsch synthetic catalyst is less than the pore volume of the second fischer-tropsch synthetic catalyst, and hydrogen contacts with the first fischer-tropsch synthetic catalyst first with CO (carbon monoxide converter) gas, contacts with the second fischer-tropsch synthetic catalyst again; The difference of the pore volume of the pore volume of the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst is 0.1-0.7 ml/g; Described the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst contain heat-resisting inorganic materials carrier and the cobalt and/or the cobalt compound that load on this carrier separately.
2. method according to claim 1, wherein, the pore volume of described the first fischer-tropsch synthetic catalyst is 0.2-0.5 ml/g, the pore volume of the second fischer-tropsch synthetic catalyst is 0.5-1 ml/g.
3. method according to claim 1, wherein, take the cumulative volume of the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst as benchmark, the loadings of described the first fischer-tropsch synthetic catalyst is 30-70 volume %, and the loadings of the second fischer-tropsch synthetic catalyst is 30-70 volume %.
4. method according to claim 1, wherein, in described the first fischer-tropsch synthetic catalyst, take the gross weight of the first fischer-tropsch synthetic catalyst as benchmark, in oxide compound, the content of cobalt is the 5-20 % by weight; In described the second fischer-tropsch synthetic catalyst, take the gross weight of the second fischer-tropsch synthetic catalyst as benchmark, in oxide compound, the content of cobalt is the 1-20 % by weight.
5. method according to claim 1, wherein, the compound of described cobalt is cobalt oxide and/or solubility cobalt salt, described heat-resisting inorganic materials is selected from one or more in aluminum oxide, pure aluminium silicate, silicon oxide, titanium oxide, zirconium white and the gac.
6. method according to claim 1, wherein, the specific surface area of the carrier of described the first fischer-tropsch synthetic catalyst and the second fischer-tropsch synthetic catalyst 100-300 meters squared per gram of respectively doing for oneself.
7. method according to claim 1, wherein, described Fischer-Tropsch synthesis condition comprises that the pressure that hydrogen contacts with CO (carbon monoxide converter) gas is the 2-4 MPa, and the temperature of contact is 180-220 ℃, and gas hourly space velocity is 400-1000 hour
-1, the raw materials components mole ratio of hydrogen and CO (carbon monoxide converter) gas is 1.8-2.2:1.
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| CN102337145B (en) * | 2010-07-22 | 2015-04-29 | 中国石油化工股份有限公司 | Fixed bed Fischer-Tropsch method for preparing liquid hydrocarbon |
| CN102911693B (en) * | 2011-08-01 | 2015-04-01 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis method by employing mixed catalyst |
| CN102911695B (en) * | 2011-08-01 | 2015-04-01 | 中国石油化工股份有限公司 | Fischer-Tropsch synthetic method of mixed system by using different catalysts |
| CN103059898B (en) * | 2011-10-24 | 2015-03-18 | 中国石油化工股份有限公司 | Method for synthesizing liquid hydrocarbons |
| CN103977801B (en) * | 2014-05-13 | 2016-02-24 | 中国科学院山西煤炭化学研究所 | A kind of high-termal conductivity Co based Fischer-Tropsch synthesis catalyst and method for making and application |
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| CN1316298A (en) * | 2000-03-02 | 2001-10-10 | 艾尼股份公司 | Load type cobalt-base catalyst |
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| CN1316298A (en) * | 2000-03-02 | 2001-10-10 | 艾尼股份公司 | Load type cobalt-base catalyst |
Non-Patent Citations (1)
| Title |
|---|
| Hualan Li.studies on cobalt catalyst supported on silica with different pore size for Fischer-Tropsch synthesis.《catalysis letters》.2006,第110卷(第1-2期),71-76. * |
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